Reaktion #4301

Reaktionsgleichung

[(4-chlorobutyl)sulfonyl]benzene

isopropylamine

→

N-(1-Methylethyl)-4-(phenylsulfonyl)-1-butanamine hydrochloride

Ausbeute 30.0%

Lösungsmittel

chloroform

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe residue obtained
2. 2
   Extraktionthe chloroform layer was extracted with water
3. 3
   TrocknenThe chloroform layer was dried
4. 4
   Filtrationfiltered
5. 5
   Sonstigesolvent removed
6. 6
   Sonstigeto give a dark brown oil
7. 7
   SonstigeThis salt was recrystallized from methanol-diethyl ether
8. 8
   Sonstigedried in vacuo overnight at 80° C

Vorschrift

A solution of 105.95 g (0.456 mole) [(4-chlorobutyl)sulfonyl]benzene was heated overnight at 75° C. on an autoclave in 200 ml of isopropylamine. The reaction mixture was stripped to dryness. The residue obtained was dissolved in chloroform and the chloroform layer was extracted with water. The chloroform layer was dried, filtered, and solvent removed to give a dark brown oil. The oil was dissolved in methanol and converted to the hydrochloride salt. This salt was recrystallized from methanol-diethyl ether and dried in vacuo overnight at 80° C. This gave white crystalline product, m.p. 155°-157.5° C. in 30% yield.

Quelle